CN109760377B - High-release-property silicon-free composite release film and preparation method thereof - Google Patents
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Abstract
The invention discloses a high-release silicon-free composite release film and a preparation method thereof, wherein the composite release film has a three-layer structure: release layer, flow layer and back layer. Wherein, lie in upper and lower top layer respectively from type layer and back layer, the mobile layer lies in from type layer and back layer between. The release layer comprises the following components in percentage by weight: 85-95% of polyphenyl ether, 5-10% of fluorine-containing polymer, 1-5% of solid lubricant and 0.5-2% of stabilizer; the flowing layer comprises the following components in percentage by weight: 50-70% of polyolefin resin, 30-50% of polyester resin and 0.5-2% of antioxidant; the back layer comprises the following components in percentage by weight: 80-95% of polyphenyl ether, 5-20% of filler and 0.5-2% of stabilizer. Through the three-layer co-casting composite process, the prepared three-layer composite release film has excellent release property, temperature resistance and glue resistance.
Description
Technical Field
The invention relates to the field of release films, in particular to a composite release film with high release property, the surface of which is not coated with any silicone oil release agent.
Background
The release film is an important auxiliary product in the production process of numerous electronic and electrical elements, can effectively improve the production efficiency of the electronic and electrical elements and improve the quality and the quality stability of products. Therefore, release films are widely used in the production of many devices such as printed circuit boards, FPC flexible circuit boards, liquid crystal polarizing plates, PDP components, organic EL components, display components, and the like.
At present, a release film which takes a polyester film as a base material and takes organosilicon materials such as silicone oil or silicone grease and the like coated on the surface as a release agent is the most widely researched and applied variety. For example, Korea Kolon Industrial Co., Ltd. coated a series of silicone compositions on a polyester film, developed a release film having good release force and antistatic property (patent application No. 201180063811.0). Also, a release film product having good release properties and little influence of atmospheric exposure was prepared by coating a cured silicone coating on a polyester film as a base material, manufactured by mitsubishi resin corporation. Generally speaking, these silicone-coated release film products have good release properties and can also withstand a certain temperature, and thus play an important role in the manufacture of many electronic devices. However, the release film has the greatest disadvantage that the silicone release agent coated on the surface of the release film has poor migration resistance, and although the release film has good release effect, the release film is easy to adhere to the surface of an electronic device during use, thereby affecting the smooth proceeding of the subsequent manufacturing process of the device. For high-end electronic devices such as flexible circuit boards, trace impurities brought in the manufacturing process can also seriously affect the quality of the devices. Particularly, with the trend of low price of electronic and electrical products in recent years, the realization of low price of related devices has become a major issue in related industries by improving the manufacturing efficiency and the yield of finished products. The high speed of device manufacturing inevitably shortens the takt time of the pressing process of electronic devices such as flexible circuit boards and the like, and the pressing temperature and pressure are obviously improved, so that higher requirements are provided for the release property, the temperature resistance and the migration resistance of the release film, which are difficult to achieve by the existing release film product. In addition, in order to avoid the phenomenon of glue overflow of the flexible circuit board and the printed circuit board in the pressing process, the performance requirement of glue resistance is also provided for the release film, and the release film is required to be capable of sinking a gap between the laminating layers in the pressing process to prevent the overflow of the adhesive. Under the circumstances, the common single-layer release film cannot meet the requirements, and the development of the silicon-free multilayer composite release film with good release property, temperature resistance and adhesive resistance is an urgent need of related industries such as circuit boards and the like.
Disclosure of Invention
Aiming at the related industry requirements and the problems of the existing release film, the invention aims to provide a silicon-free multilayer composite release film product which meets the related industry requirements of a flexible circuit board and has good release property, temperature resistance and glue resistance and a preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: the utility model provides a high release does not have silicon composite from type membrane, from type membrane form by three-layer complex: the release layer, the flow layer and the back layer; wherein, lie in upper and lower top layer respectively from type layer and back layer, the mobile layer lies in from type layer and back layer between.
The release layer comprises the following components in percentage by weight: 85-95% of polyphenyl ether, 5-10% of fluorine-containing polymer, 1-5% of solid lubricant and 0.5-2% of stabilizer.
The polyphenyl ether in the invention has a chemical name of poly 2, 6-dimethyl-1, 4-phenyl ether, PPO or PPE for short, is an engineering plastic with excellent comprehensive performance, and has outstanding heat resistance and a melting point as high as 270 ℃; in addition, the polyphenyl ether has excellent water resistance, wear resistance and dimensional stability, the surface energy of the polyphenyl ether is lower, and the adhesion to other materials is smaller; therefore, in the technical scheme of the invention, the polyphenyl ether is selected as the base resin of the release layer.
The fluorine-containing polymer in the invention is one or a mixture of more of polytetrafluoroethylene, polyvinylidene fluoride, polyhexafluoropropylene and fluorine 46; the fluorine-containing polymers have excellent heat resistance and non-stick property, and can effectively improve the heat resistance and release property of the release layer when being added into polyphenyl ether base resin.
The solid lubricant is one or a mixture of molybdenum disulfide, graphite, graphene and boron nitride; the inorganic solids are flaky two-dimensional or flaky three-dimensional materials, have very good lubricating and antifriction functions, and can reduce the friction coefficient of the release layer and reduce the peeling force when being added into the release layer; in addition, in the casting process of the film, the inorganic lubricating materials still keep a solid particle state due to high melting point, so that certain roughness is formed on the surface of the release layer, and the surface smoothness of the release layer is further improved.
The average particle size of the solid lubricant is 50-800 nm, preferably 100-600 nm, most preferably 100-300 nm, and the average particle size is too small, so that the particles are easy to agglomerate and difficult to disperse uniformly; the average particle size is too large, so that the surface of the release layer is too rough, and bad marks are easily caused on the surface of a device product when the release film is used.
The stabilizer is one or a mixture of more of tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, N-octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate, 2, 6-di-tert-butyl-4-methylphenol, N, N' -bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexanediamine, triphenyl phosphite, diisooctyl monobenzene phosphite, diisooctyl diphenyl phosphite and tris [2, 4-di-tert-butylphenyl ] phosphite; these compounds can be used alone or in combination, and can block the chain-type degradation reaction of free radicals generated by the action of heat and oxygen in the high molecular material, thereby avoiding or reducing the decomposition of the polymer in the molding process and keeping the original excellent performance.
The flowing layer comprises the following components in percentage by weight: 50-70% of polyolefin resin, 30-50% of polyester resin and 0.5-2% of antioxidant.
The polyolefin resin in the invention is one or a mixture of more of polyethylene, polypropylene and metallocene catalyzed ethylene-octene copolymer; the melting points of the polyolefin resins are all 150 ℃, the polyolefin resins are melted into liquid under the circuit board laminating process condition, and the non-polar high polymers have small intermolecular acting force and good melt fluidity and can play a good role in preventing glue overflow in the laminating process.
The polyester resin is one or a mixture of a plurality of polyethylene glycol terephthalate, polybutylene terephthalate, ethylene-vinyl acetate copolymer, ethylene-methyl methacrylate copolymer and ethylene-butyl methacrylate copolymer; the polyester material has good flexibility and elasticity, and besides the function of assisting the polyolefin material to provide the flow glue resistance in the pressing process, the polyester material also has the function of enabling the film to have better flexibility and elasticity at normal temperature and normal pressure, and is convenient for the operations of winding, spreading and the like of the release film.
The back layer comprises the following components in percentage by weight: 80-95% of polyphenyl ether, 5-20% of filler and 0.5-2% of stabilizer.
The filler in the invention is one or more of calcium carbonate, silicon dioxide, mica powder, diatomite and montmorillonite; the inorganic fillers have good heat resistance, and can improve the temperature resistance of the back layer; in addition, the inorganic fillers are low in price, so that the cost of the release film can be reduced.
In the high-release silicon-free composite release film, the thickness of the release layer is 10-30 microns, the thickness of the flowing layer is 30-70 microns, and the thickness of the back layer is 30-70 microns.
The invention relates to a preparation method of a high-release silicon-free composite release film, which comprises the following operation steps:
1) putting the components in the separation layer into an internal mixer according to the mass ratio, and premixing at normal temperature for 3-6 min; then drying the premix in a dryer at the temperature of 120-140 ℃ for 2-4 hours, and then performing melt blending by adopting a double-screw extruder, controlling the temperature of the screws at the temperature of 280-320 ℃, and extruding and granulating the mixture;
2) putting the components in the flowing layer into an internal mixer according to the mass ratio, and premixing at normal temperature for 3-6 min; then the premix is dried in a vacuum drier for 2 to 4 hours at the temperature of between 50 and 80 ℃, and then a double-screw extruder is adopted for melt blending, the temperature of the screws is controlled at 260 ℃ and 150 ℃, and the mixture is extruded and granulated;
3) putting the components in the back layer into an internal mixer according to the mass ratio, and premixing at normal temperature for 3-6 min; then drying the premix in a dryer at the temperature of 120-140 ℃ for 2-4 hours, and then performing melt blending by adopting a double-screw extruder, controlling the temperature of the screws at the temperature of 280-320 ℃, and extruding and granulating the mixture;
4) and adding the release layer granules, the middle layer granules and the back layer granules which are prepared by blending into a three-layer extrusion co-casting machine set, and casting and compounding the three granules into a film in an extrusion casting compounding film forming mode to obtain the high-release silicon-free composite release film product.
The invention has the advantages that: the release film with a three-layer composite structure of a release layer, a flow layer and a back layer is prepared by a three-layer co-casting composite process, wherein the release layer takes high-temperature-resistant and low-surface-energy polyphenyl ether as a substrate, and is matched with fluororesin and a solid lubricant with good lubricating property and heat resistance, so that the release layer has excellent temperature resistance and release property; the middle layer is formed by mixing a polyolefin material with good melt fluidity and a polyester material, so that the release film is endowed with good glue overflow prevention performance; the back layer adopts the cooperation of polyphenyl ether and heat-resisting inorganic filler, when improving its temperature resistance, the cost is reduced, is favorable to the popularization of product, and the design of three-layer composite structure, every layer of film do its job respectively to make the compound type membrane have excellent type nature, temperature resistance and hinder gluey nature simultaneously, satisfy trades such as current circuit board to the high requirement from type membrane.
Drawings
Fig. 1 is a schematic structural view of the high release silicon-free composite release film of the present invention.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The invention can be further clearly understood by means of the specific examples of the invention given below:
example one
A high-release silicon-free composite release film comprises the following components in percentage by weight: 85% of polyphenyl ether, 5% of polytetrafluoroethylene, 5% of polyhexafluoropropylene, 3% of molybdenum disulfide and 2% of tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester; the flowing layer comprises the following components in percentage by weight: 50% of polyethylene, 49% of ethylene-methyl acrylate copolymer and 1% of tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester; the back layer comprises the following components in percentage by weight: 80 percent of polyphenyl ether, 19 percent of calcium carbonate and 1 percent of [ x1] - (3, 5-di-tert-butyl-4-hydroxyphenyl) n-octadecyl propionate.
The preparation method comprises the following operation steps:
1) putting the components in the separation layer into an internal mixer according to the mass ratio, and premixing at normal temperature for 5 min; then drying the premix in a dryer at 140 ℃ for 2 hours, and then carrying out melt blending by adopting a double-screw extruder, controlling the temperature of screws at 320 ℃, and extruding and granulating the mixture;
2) putting the components in the flowing layer into an internal mixer according to the mass ratio, and premixing at normal temperature for 5 min; then the premix is dried in a vacuum drier for 3 hours at 60 ℃ in vacuum, and then is melted and blended by a double-screw extruder, the temperature of the screw is controlled at 160 ℃, and the mixture is extruded and granulated;
3) putting the components in the back layer into an internal mixer according to the mass ratio, and premixing at normal temperature for 5 min; then drying the premix in a dryer at 140 ℃ for 2 hours, and then carrying out melt blending by adopting a double-screw extruder, controlling the temperature of screws at 300 ℃, and extruding and granulating the mixture;
4) and adding the release layer granules, the middle layer granules and the back layer granules which are prepared by blending into a three-layer extrusion co-casting machine set, and casting and compounding the three granules into a film in an extrusion casting compounding film forming mode to obtain the high-release silicon-free composite release film product.
Example two
A high-release silicon-free composite release film comprises the following components in percentage by weight: 90% of polyphenyl ether, 3% of polyhexafluoropropylene, 3% of fluorine 463%, 3% of graphite, 0.5% of tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester and 0.5% of tri [ 2.4-di-tert-butylphenyl ] phosphite; the flowing layer comprises the following components in percentage by weight: 30% of polyethylene, 20% of POM, 49% of ethylene-vinyl acetate copolymer and 1% of pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ]; the back layer comprises the following components in percentage by weight: 85 percent of polyphenyl ether, 14 percent of calcium carbonate and 1 percent of [ x2] - (3, 5-di-tert-butyl-4-hydroxyphenyl) n-octadecyl propionate.
The preparation method comprises the following operation steps:
1) putting the components in the separation layer into an internal mixer according to the mass ratio, and premixing at normal temperature for 4 min; then drying the premix in a dryer at 130 ℃ for 3 hours, and then carrying out melt blending by adopting a double-screw extruder, controlling the temperature of screws at 310 ℃, and extruding and granulating the mixture;
2) putting the components in the flowing layer into an internal mixer according to the mass ratio, and premixing at normal temperature for 5 min; then the premix is dried in a vacuum drier for 4 hours at 50 ℃ in vacuum, and then is melted and blended by a double-screw extruder, the temperature of the screw is controlled at 180 ℃, and the mixture is extruded and granulated;
3) putting the components in the back layer into an internal mixer according to the mass ratio, and premixing at normal temperature for 5 min; then drying the premix in a dryer at 140 ℃ for 2 hours, and then carrying out melt blending by adopting a double-screw extruder, controlling the temperature of screws at 300 ℃, and extruding and granulating the mixture;
4) and adding the release layer granules, the middle layer granules and the back layer granules which are prepared by blending into a three-layer extrusion co-casting machine set, and casting and compounding the three granules into a film in an extrusion casting compounding film forming mode to obtain the high-release silicon-free composite release film product.
EXAMPLE III
A high-release silicon-free composite release film comprises the following components in percentage by weight: 95% of polyphenyl ether, 462.5% of fluorine, 2% of graphene and 0.5% of tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester; the flowing layer comprises the following components in percentage by weight: 25% of polyethylene, 10% of polypropylene, 15% of POM (polyoxymethylene), 49% of ethylene-butyl acrylate copolymer and 1% of pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ]; the back layer comprises the following components in percentage by weight: 90 percent of polyphenyl ether, 9 percent of calcium carbonate, 0.5 percent of [ x3] - (3, 5-di-tert-butyl-4-hydroxyphenyl) n-octadecyl propionate and 0.5 percent of 2, 6-di-tert-butyl-4-methylphenol.
The preparation method comprises the following operation steps:
1) putting the components in the separation layer into an internal mixer according to the mass ratio, and premixing at normal temperature for 3 min; then drying the premix in a dryer at 120 ℃ for 4 hours, and then carrying out melt blending by adopting a double-screw extruder, controlling the temperature of screws at 300 ℃, and extruding and granulating the mixture;
2) putting the components in the flowing layer into an internal mixer according to the mass ratio, and premixing at normal temperature for 6 min; then the premix is dried in a vacuum dryer at 70 ℃ for 3 hours in vacuum, and then a double-screw extruder is adopted for melt blending, the temperature of the screw is controlled at 200 ℃, and the mixture is extruded and granulated;
3) putting the components in the back layer into an internal mixer according to the mass ratio, and premixing at normal temperature for 5 min; then drying the premix in a dryer at 140 ℃ for 2 hours, and then carrying out melt blending by adopting a double-screw extruder, controlling the temperature of screws at 290 ℃, and extruding and granulating the mixture;
4) and adding the release layer granules, the middle layer granules and the back layer granules which are prepared by blending into a three-layer extrusion co-casting machine set, and casting and compounding the three granules into a film in an extrusion casting compounding film forming mode to obtain the high-release silicon-free composite release film product.
The performance parameters of the composite release film obtained by adopting the formula and the method are as follows:
tensile strength: not less than 23MPa
Impact strength: not less than 120J/m
Rate of change in size: less than or equal to 0.6 percent
Wrinkle occurrence rate: less than or equal to 1 percent
Porosity formation rate: less than or equal to 1 percent
The use temperature is as follows: not less than 200 DEG C
Glue overflow length: less than or equal to 1mm
Surface energy: less than or equal to 32 dynes/cm
The invention provides a thought and a method for preparing a high-release silicon-free composite release film, and particularly provides a plurality of methods and ways for realizing the technical scheme.
Claims (9)
1. The utility model provides a high compound from type membrane of type nature silicon-free which characterized in that, from type membrane form by the three-layer complex: the release layer, the flow layer and the back layer; the release layer and the back layer are respectively positioned on the upper surface layer and the lower surface layer, and the flowing layer is positioned between the release layer and the back layer;
the release layer comprises the following components in percentage by weight: 85-95% of polyphenyl ether, 5-10% of fluorine-containing polymer, 1-5% of solid lubricant and 0.5-2% of stabilizer;
the flowing layer comprises the following components in percentage by weight: 50-70% of polyolefin resin, 30-50% of polyester resin and 0.5-2% of antioxidant; the back layer comprises the following components in percentage by weight: 80-95% of polyphenyl ether, 5-20% of filler and 0.5-2% of stabilizer;
in the high-release silicon-free composite release film, the thickness of a release layer is 10-30 microns, the thickness of a flowing layer is 30-70 microns, and the thickness of a back layer is 30-70 microns.
2. The high-release silicon-free composite release film according to claim 1, wherein the fluorine-containing polymer is one or a mixture of polytetrafluoroethylene, polyvinylidene fluoride, polyhexafluoropropylene and fluorine 46.
3. The high-release silicon-free composite release film according to claim 1, wherein the solid lubricant is one or a mixture of molybdenum disulfide, graphite, graphene and boron nitride.
4. The high-release silicon-free composite release film according to claim 1, wherein the particle size of the solid lubricant is 50-800 nm.
5. The high release silicon-free composite release film according to claim 1, wherein the stabilizer is one or more of tetra [ β - ([ x1] -di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, N-octadecyl β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate, 2, 6-di-tert-butyl-4-methylphenol, N' -bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexanediamine, triphenyl phosphite, diisooctyl monobenzene phosphite, diisooctyl diphenyl phosphite, and tris [2, 4-di-tert-butylphenyl ] phosphite.
6. The high-release silicon-free composite release film according to claim 1, wherein the polyolefin resin is one or a mixture of polyethylene, polypropylene and metallocene-catalyzed ethylene-octene copolymer.
7. The high-release silicon-free composite release film according to claim 1, wherein the polyester resin is one or a mixture of polyethylene terephthalate, polybutylene terephthalate, ethylene-vinyl acetate copolymer, ethylene-methyl methacrylate copolymer and ethylene-butyl methacrylate copolymer.
8. The high-release silicon-free composite release film according to claim 1, wherein the filler is one or more of calcium carbonate, silica, mica powder, diatomite and montmorillonite.
9. The preparation method of the high-release silicon-free composite release film according to claim 1, comprising the following steps:
1) putting the components in the separation layer into an internal mixer according to the mass ratio, and premixing at normal temperature for 3-6 min; then drying the premix in a dryer at the temperature of 120-140 ℃ for 2-4 hours, and then performing melt blending by adopting a double-screw extruder, controlling the temperature of the screws at the temperature of 280-320 ℃, and extruding and granulating the mixture;
2) putting the components in the flowing layer into an internal mixer according to the mass ratio, and premixing at normal temperature for 3-6 min; then the premix is dried in a vacuum drier for 2 to 4 hours at the temperature of between 50 and 80 ℃, and then a double-screw extruder is adopted for melt blending, the temperature of the screws is controlled at 260 ℃ and 150 ℃, and the mixture is extruded and granulated;
3) putting the components in the back layer into an internal mixer according to the mass ratio, and premixing at normal temperature for 3-6 min; then drying the premix in a dryer at the temperature of 120-140 ℃ for 2-4 hours, and then performing melt blending by adopting a double-screw extruder, controlling the temperature of the screws at the temperature of 280-320 ℃, and extruding and granulating the mixture;
4) and adding the release layer granules, the middle layer granules and the back layer granules which are prepared by blending into a three-layer extrusion co-casting machine set, and casting and compounding the three granules into a film in an extrusion casting compounding film forming mode to obtain the high-release silicon-free composite release film product.
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| CN110193982B (en) * | 2019-05-29 | 2021-03-30 | 珠海市一心材料科技有限公司 | High-temperature glue-resistant film and manufacturing method thereof |
| CN110239185B (en) * | 2019-06-14 | 2021-05-11 | 江苏双星彩塑新材料股份有限公司 | MLCC release film base film and preparation method thereof |
| CN110358126A (en) * | 2019-07-22 | 2019-10-22 | 安徽屹珹新材料科技有限公司 | A kind of high temperature resistant resistance glue release film and its preparation method and application for flexible circuit board |
| CN111002667B (en) * | 2019-12-19 | 2022-03-08 | 宁波长阳科技股份有限公司 | Release film and preparation method thereof |
| CN113067020B (en) * | 2021-03-29 | 2022-07-15 | 浙江汉丞新能源有限公司 | Composite membrane electrode of high-enhancement type fluorine-containing proton or ion exchange membrane |
| JP2024515480A (en) * | 2021-03-29 | 2024-04-10 | 浙江漢丞新能源有限公司 | Special highly reinforced fluorine-containing proton or ion exchange membrane composite membrane, composite membrane electrode, special highly reinforced fluorine-chlorine-containing alkaline battery membrane, special release membrane, and methods for producing the same |
| CN113416503A (en) * | 2021-04-29 | 2021-09-21 | 江苏双星彩塑新材料股份有限公司 | Online coating low-peeling-force polyester release film and preparation method thereof |
| CN113352715A (en) * | 2021-04-29 | 2021-09-07 | 江苏双星彩塑新材料股份有限公司 | PET matte composite release film and preparation method thereof |
| CN113263816A (en) * | 2021-05-22 | 2021-08-17 | 江苏双星彩塑新材料股份有限公司 | Impact-resistant and explosion-proof polyester release film and preparation method thereof |
| CN113388138A (en) * | 2021-06-24 | 2021-09-14 | 扬州万润光电科技有限公司 | High-temperature stable release film and preparation method thereof |
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| CN105802157B (en) * | 2016-05-16 | 2018-01-23 | 久裕电子科技（江苏）有限公司 | A kind of high temperature mould release membrance and its production technology |
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